CN105420751A - Method for preparing hydrocarbon through electrochemical reduction of carbon dioxide - Google Patents
Method for preparing hydrocarbon through electrochemical reduction of carbon dioxide Download PDFInfo
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- CN105420751A CN105420751A CN201410491284.9A CN201410491284A CN105420751A CN 105420751 A CN105420751 A CN 105420751A CN 201410491284 A CN201410491284 A CN 201410491284A CN 105420751 A CN105420751 A CN 105420751A
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Abstract
The invention relates to a method for preparing hydrocarbon through electrochemical reduction of carbon dioxide. An electrolytic tank is divided into a left cavity and a right cavity through a proton exchange membrane, the left cavity and the right cavity are not communicated with each other, and the two cavities serve as a cathode chamber and an anode chamber respectively; and the cathode chamber is filled with an electrolyte solution, the electrolyte solution is an inorganic electrolyte aqueous solution where the carbon dioxide is dissolved, and an organic solvent is further added into the electrolyte solution. The method of combining inorganic salts and the organic solvent is adopted, and metal Cu electrodes in different shapes and forms serve as cathodes, anodes are formed by Pt pieces or Pt wire electrodes and the like, and therefore the conversion rate of the carbon dioxide and the energy cycle utilization rate are greatly increased.
Description
Technical field
The present invention relates to electrochemically reducing carbon dioxide technology, belong to Resources of Carbon Dioxide and utilize field.
Background technology
Fixing and the conversion of CO2 is one of effective measure reducing CO2 discharge capacity.It mainly comprises seals fixing, shortening, catalytic reforming and electrochemical conversion method up for safekeeping.Traditional shortening, catalystic reforming method just can must carry out under high temperature, high pressure or catalysts conditions, and low-conversion and efficiency all limit its large-scale application.The advantage of electrochemical reducing is the high redox potential (-1.9Vvs.SHE) that effectively can overcome CO2/CO2-, gets final product realization response under normal temperature and pressure, and reaction conditions is gentle, simple to operate; And the selectivity synthesis to product is realized by control electrode and reaction conditions in electro-reduction process.Therefore relative to other method of reducing, electrochemical reduction CO2 has better application prospect.
Electrochemical reduction CO2 (ERC) technology utilizes electric energy that CO2 is reduced to chemical, realizes a kind of technology of CO2 recycling.Along with the fast development of renewable energy technologies, cost of electricity-generating will significantly decline.Utilize renewable energy power generation, by electrochemical techniques make CO2 directly and H2O react and generate organic compound, as CH3OH, CH4 and hydrocarbon compound etc., realize electric energy to chemical transformation of energy, not only make ERC technology have more economy, the storage of renewable energy source can also be realized, and form a carbon and Conversion of energy circulation.Compared with other CO2 transformation technologies, the sharpest edges of ERC technology are to utilize water as the hydrogen source of reaction, and normal temperature and pressure can realize the Efficient Conversion of CO2, therefore do not need hydrogen manufacturing and heat, pressurize the required extra energy consumed, total energy consumption is lower, and facility investment is few.Thus, it has potential economic benefit and environmental benefit, causes people's extensive concern.Someone expects, following CO2 chemical will become new organic chemical industry's system, and its development is significant to the energy and environmental problem that solve facing mankind.
The kind of reduzate of ERC reaction on the catalyzer of differing materials, transformation efficiency, current efficiency are different.High hydrogen-evolution overpotential material (as Pb, In and Sn), electroreduction CO2 can obtain formate or carboxylic acid product, and part report shows that current efficiency is up to 100% on Pb diffusion electrode, but pattern, structural changes [Machunda, R.L. occur Pb; Lee, J.Surf.Interface.Anal., 2010,42 (6-7), 564-567.].Take Fe/CNT as electrode materials, principal product is Virahol, but productivity ratio Pt/CNT improves [Arrigo, R. greatly; Schuster, M.E.; Sabine, W.; Etal.Chemsuschem., 2012,5 (3), 577.].[Wu, J.W., Risalvato, the F.G. such as Wu; Etal., J.Electrochem.Soc., 2012,159 (7) F353] to have studied with Sn be the performance of catalyst preparing formate.Research shows that Falady efficiency in-1.7V (vsSCE), 0.1MNa2SO4 solution is up to nearly 95%.0.5MKHCO3 both can produce at a high speed the best ionogen that formate keeps the faradic efficiency of about 63% simultaneously, and the generating rate of-2.0V reaches 3.8umolmin-1cm-2.Relative to other materials, Cu catalysis carbonic acid gas is shaped with organic compounds, and especially methane and hydro carbons have higher faradic efficiency.Thus the research emphasis of ERC technology is become.But be electrolytical carbonic acid gas hydrocarbon polymer with the aqueous solution, liberation of hydrogen side reaction is serious, and reacted current potential is larger, faradic efficiency but generally all less than 40%.In addition, carbonic acid gas solubleness is in aqueous less, causes cathodic reaction speed slower.201110078444.3 adopt organic solvent/ionic liquid solution, improve the solubleness of CO2 to a certain extent, improve the faradic efficiency of reaction.But ionic liquid costly, and ionic liquid needs the good effect of competence exertion in the environment of complete non-water.If in atmosphere, ionic liquid easily absorbs water, and its performance is significantly reduced, and is difficult to significantly be applied in air ambient.
Summary of the invention
The object of the invention is to the shortcoming overcoming above-mentioned pure water solution and ionic liquid solution, the method adopting inorganic salts and organic solvent phase compound is proposed, utilize different-shape Ni metal electrode as negative electrode, anode adopts Pt sheet or Pt silk electrode etc., and the efficiency making Carbon dioxide electrochemical reduction prepare hydrocarbon polymer (CH4/C2H6/C2H4) etc. improves 10%-50%.
Electrochemically reducing carbon dioxide prepares a method for hydrocarbon polymer, and by proton exchange membrane, electrolyzer is divided into two the mutual disconnected chambers in left and right, two chambers are respectively as cathode compartment and anolyte compartment; The electrolyte solution loaded in cathode compartment is: the inorganic electrolyte aqueous solution being dissolved with carbonic acid gas, is wherein also added with organic solvent; The volume ratio of inorganic electrolyte and organic solvent is 20:1 ~ 1:2; Inorganic electrolyte is one or two or more kinds in alkaline carbonate, alkali metal hydrocarbonate, alkali metal sulfates, alkali metal phosphate, alkali metal hydrogen phosphate, and organic solvent is one or two or more kinds in methyl alcohol, ethanol, Virahol, ethylene glycol, tetrahydrofuran (THF), dimethyl sulfoxide (DMSO), dimethyl formamide, N-Methyl pyrrolidone; The aqueous solution containing supporting electrolyte is injected with in anolyte compartment;
Negative electrode adopts Cu electrode; Anode adopts Pt plate electrode or Pt silk electrode; Negative electrode is as working electrode, and apply-1.5V ~-4V voltage at negative electrode, be the mixture of hydrocarbon polymer and hydrogen by carbon dioxide reduction, hydrocarbon polymer is one or two or more kinds in methane, ethane, ethene.
Concrete technological process is as follows:
At room temperature, catholyte solution is injected cathode compartment, electrolyte solution is passed into CO2 gas, carbonic acid gas is absorbed; Meanwhile, the aqueous solution containing supporting electrolyte is injected in anolyte compartment, as anolyte compartment's electrolytic solution;
At ambient temperature, connect electrolysis power, carry out electrolytic reaction, anode generation oxygen evolution reaction, the Hydrogen Proton of generation arrives negative electrode by conductive membranes, on negative electrode, electro-reduction reaction occurs with carbonic acid gas, the mixture of Formed hydrogen compound and hydrogen;
At cathode compartment upper collection gaseous product, obtain the mixture of hydrocarbon polymer and hydrogen.
Described cathode electrode is Cu electrode, and Cu electrode is one or two or more kinds in foam Cu, Cu plate, Cu sheet, Cu paper tinsel, Cu net, nanometer Cu whisker, Cu nano wire, Cu nano particle, CuCl, CuBr.
Supporting electrolyte in anolyte compartment's aqueous solution is any one in sodium bicarbonate, saleratus, sodium hydrogen phosphate, potassium hydrogen phosphate, SODIUM PHOSPHATE, MONOBASIC, potassium primary phosphate, sodium pyrosulfate, sal enixum or sulfuric acid, and its concentration in water is 0.1-3mol/L.
Basic metal is any one or more than two kinds in Li, K, Na; The volumetric molar concentration 0.05-2mol/L of the inorganic electrolyte aqueous solution.
In electro-reduction process, anode is as to electrode, and negative electrode applies to be the voltage of-1.5V to-4.0V relative to the saturated KCl reference electrode of Hg/Hg2Cl2/.
Electric energy wherein for the electrochemical reduction of described carbonic acid gas is provided by the renewable energy source based on nuclear energy, water power energy, wind energy or sun power.
The present invention compared with prior art has following beneficial effect:
The organic solvent that the present invention adopts, as methyl alcohol, ethanol, Virahol, ethylene glycol, tetrahydrofuran (THF), dimethyl sulfoxide (DMSO), dimethyl formamide, N-Methyl pyrrolidone, it is conventional organism, price is low, simple and easy to get, and there is good dispersiveness in water, not only can improve carbonic acid gas solubleness in the electrolytic solution, also can reduce the efficiency of liberation of hydrogen side reaction, improve the faradic efficiency of hydrocarbon polymer.
Negative electrode adopts the Cu electrode of different-shape, can regulate and control the faradic efficiency of hydrocarbon polymer, reduce reacted current potential;
Embodiment
Application
By made electrode, as carbon dioxide reduction hydrocarbon polymer negative electrode.And carry out electro-chemical test by three-electrode system:
Working electrode: the electrode prepared by the present invention; Be Pt sheet to electrode, reference electrode is the saturated KCl of Hg/Hg2Cl2/ (SCE).Working electrode and be 0.5cm to the distance between electrode, adopts salt bridge to reduce liquid potential.CO2 flow under meter controls, and flow velocity is 60ml/min.
The method that table 1. embodiment of the present invention 1 and comparative example adopt, carbon dioxide conversion is the efficiency comparative of hydrocarbon polymer
| Sample ID | Methane faradic efficiency | Ethene faradic efficiency |
| Embodiment 1 | 65.0％ | 5％ |
| Embodiment 2 | 34％ | 8％ |
| Comparative example 1 | 55％ | 2％ |
Embodiment 1
At room temperature, the mixed solution of catholyte solution 0.5MKHCO3 aqueous solution 100ml and 5ml methanol solution (is injected cathode compartment, electrolyte solution passed into CO2 gas, absorb carbonic acid gas; Meanwhile, the 0.1MH2SO4 aqueous solution is injected in anolyte compartment, as anolyte compartment's electrolytic solution; Utilize Cu paper tinsel (thickness 0.01mm) as negative electrode Cu electrode, Pt sheet is as anode electrode; At ambient temperature, connect electrolysis power, carrying out electrolytic reaction at-2.0Vvs.SCE, anode generation oxygen evolution reaction, the Hydrogen Proton of generation arrives negative electrode by conductive membranes, on negative electrode, electro-reduction reaction occurs with carbonic acid gas, Formed hydrogen compound gas; At cathode compartment upper collection gaseous product, obtain the mixture of the product such as methane and ethene;
Embodiment 2
At room temperature, the mixed solution of catholyte solution 0.2NaKHCO3 aqueous solution 100ml and 5ml aqueous isopropanol (is injected cathode compartment, electrolyte solution passed into CO2 gas, absorb carbonic acid gas; Meanwhile, the 0.1MNaHCO3 aqueous solution is injected in anolyte compartment, as anolyte compartment's electrolytic solution; Utilize Cu paper tinsel (thickness 0.02mm) as negative electrode Cu electrode, Pt sheet is as anode electrode; At ambient temperature, connect electrolysis power, carrying out electrolytic reaction at-2.5Vvs.SCE, anode generation oxygen evolution reaction, the Hydrogen Proton of generation arrives negative electrode by conductive membranes, on negative electrode, electro-reduction reaction occurs with carbonic acid gas, Formed hydrogen compound gas; At cathode compartment upper collection gaseous product, obtain the mixture of the products such as methane, ethane, ethene;
Embodiment 3
At room temperature, the mixed solution of catholyte solution 0.2Na2SO4 aqueous solution 50ml and 5ml propylene glycol solution (is injected cathode compartment, electrolyte solution passed into CO2 gas, absorb carbonic acid gas; Meanwhile, the 0.1MNaHCO3 aqueous solution is injected in anolyte compartment, as anolyte compartment's electrolytic solution; Utilize Cu net (thickness 0.125mm) as negative electrode Cu electrode, Pt silk is as anode electrode; At ambient temperature, connect electrolysis power, carrying out electrolytic reaction at-2.5Vvs.SCE, anode generation oxygen evolution reaction, the Hydrogen Proton of generation arrives negative electrode by conductive membranes, on negative electrode, electro-reduction reaction occurs with carbonic acid gas, Formed hydrogen compound gas; At cathode compartment upper collection gaseous product, obtain the mixture of the products such as methane, ethane, ethene;
Embodiment 4
At room temperature, the mixed solution of catholyte solution 0.5Na2SO4 aqueous solution 200ml and 5mlN-methyl-2-pyrrolidone is injected cathode compartment, electrolyte solution is passed into CO2 gas, carbonic acid gas is absorbed; Meanwhile, the 0.1MH2SO4 aqueous solution is injected in anolyte compartment, as anolyte compartment's electrolytic solution; Utilize Cu net (thickness 0.125mm) as negative electrode Cu electrode, Pt sheet is as to electrode; At ambient temperature, connect electrolysis power, carrying out electrolytic reaction at-2.0Vvs.SCE, anode generation oxygen evolution reaction, the Hydrogen Proton of generation arrives negative electrode by conductive membranes, on negative electrode, electro-reduction reaction occurs with carbonic acid gas, Formed hydrogen compound gas; At cathode compartment upper collection gaseous product, obtain the mixture of the products such as methane, ethane, ethene;
Comparative example 1
At room temperature, catholyte solution 0.5MKHCO3a aqueous solution 100ml solution is injected cathode compartment, electrolyte solution is passed into CO2 gas, carbonic acid gas is absorbed; Meanwhile, the 0.1MH2SO4 aqueous solution is injected in anolyte compartment, as anolyte compartment's electrolytic solution; Utilize Cu paper tinsel (thickness 0.01mm) as negative electrode Cu electrode, Pt sheet is as anode electrode; At ambient temperature, connect electrolysis power, carrying out electrolytic reaction at-2.0Vvs.SCE, anode generation oxygen evolution reaction, the Hydrogen Proton of generation arrives negative electrode by conductive membranes, on negative electrode, electro-reduction reaction occurs with carbonic acid gas, Formed hydrogen compound gas; At cathode compartment upper collection gaseous product, obtain the mixture of the products such as methane, ethane, ethene.
Application
By made electrode, as carbon dioxide reduction hydrocarbon polymer negative electrode.And carry out electro-chemical test by three-electrode system:
Working electrode: the electrode prepared by the present invention; Be Pt sheet to electrode, reference electrode is the saturated KCl of Hg/Hg2Cl2/ (SCE).Working electrode and be 0.5cm to the distance between electrode, adopts salt bridge to reduce liquid potential.CO2 flow under meter controls, and flow velocity is 60ml/min.The method that table 1. embodiment of the present invention 1 and comparative example adopt, carbon dioxide conversion is the efficiency comparative of hydrocarbon polymer
| Sample ID | Methane faradic efficiency | Ethene faradic efficiency |
| Embodiment 1 | 65.0％ | 5％ |
| Embodiment 2 | 34％ | 8％ |
| Comparative example 1 | 55％ | 2％ |
Show in table 1, CH in embodiment 1 and embodiment 2
4faradic efficiency be obviously better than the faradic efficiency of the method described in comparative example 1, this illustrates that the efficiency that method of the present invention makes electrochemical reaction be converted into hydrocarbon polymer is significantly improved.
Claims (7)
1. electrochemically reducing carbon dioxide prepares a method for hydrocarbon polymer, it is characterized in that:
By proton exchange membrane, electrolyzer is divided into two the mutual disconnected chambers in left and right, two chambers are respectively as cathode compartment and anolyte compartment;
The electrolyte solution loaded in cathode compartment is: the inorganic electrolyte aqueous solution being dissolved with carbonic acid gas, is wherein also added with organic solvent; The volume ratio of the inorganic electrolyte aqueous solution and organic solvent is 20:1 ~ 1:2; Inorganic electrolyte is one or two or more kinds in alkaline carbonate, alkali metal hydrocarbonate, alkali metal sulfates, alkali metal phosphate, alkali metal hydrogen phosphate, and organic solvent is one or two or more kinds in methyl alcohol, ethanol, Virahol, ethylene glycol, tetrahydrofuran (THF), dimethyl sulfoxide (DMSO), dimethyl formamide, N-Methyl pyrrolidone;
The aqueous solution containing supporting electrolyte is injected with in anolyte compartment;
Negative electrode adopts Cu electrode; Anode adopts Pt plate electrode or Pt silk electrode; Negative electrode is as working electrode, and apply-1.5V ~-4V voltage at negative electrode, be the mixture of hydrocarbon polymer and hydrogen by carbon dioxide reduction, hydrocarbon polymer is one or two or more kinds in methane, ethane, ethene.
2. method according to claim 1, is characterized in that: concrete technological process is as follows:
1) at room temperature, catholyte solution is injected cathode compartment, electrolyte solution is passed into CO
2gas, absorbs carbonic acid gas; Meanwhile, the aqueous solution containing supporting electrolyte is injected in anolyte compartment, as anolyte compartment's electrolytic solution;
2) at ambient temperature, connect electrolysis power, carry out electrolytic reaction, anode generation oxygen evolution reaction, the Hydrogen Proton of generation arrives negative electrode by conductive membranes, on negative electrode, electro-reduction reaction occurs with carbonic acid gas, the mixture of Formed hydrogen compound and hydrogen;
3) at cathode compartment upper collection gaseous product, the mixture of hydrocarbon polymer and hydrogen is obtained.
3. method according to claim 1, it is characterized in that: described cathode electrode is Cu electrode, Cu electrode is one or two or more kinds in foam Cu, Cu plate, Cu sheet, Cu paper tinsel, Cu net, nanometer Cu whisker, Cu nano wire, Cu nano particle, CuCl, CuBr.
4. method according to claim 1, it is characterized in that: the supporting electrolyte in anolyte compartment's aqueous solution is any one in sodium bicarbonate, saleratus, sodium hydrogen phosphate, potassium hydrogen phosphate, SODIUM PHOSPHATE, MONOBASIC, potassium primary phosphate, sodium pyrosulfate, sal enixum or sulfuric acid, its concentration in water is 0.1-3mol/L.
5. method according to claim 1, is characterized in that: basic metal is any one or more than two kinds in Li, K, Na; The volumetric molar concentration 0.05-2mol/L of the inorganic electrolyte aqueous solution.
6. method according to claim 1, is characterized in that: in electro-reduction process, and anode is as to electrode, and negative electrode applies relative to Hg/Hg
2cl
2/ saturated KCl reference electrode is the voltage of-1.5V to-4.0V.
7. method according to claim 1, is characterized in that: the electric energy wherein for the electrochemical reduction of described carbonic acid gas is provided by the renewable energy source based on nuclear energy, water power energy, wind energy or sun power.
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| CN108118361A (en) * | 2016-11-26 | 2018-06-05 | 中国科学院大连化学物理研究所 | A kind of raising CO2The method of electrochemical reduction electrode catalytic activity |
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| CN114000172B (en) * | 2021-12-16 | 2023-03-07 | 东北大学 | Method for trapping and reducing carbon dioxide and co-producing oxygen or chlorine |
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